2-Nitroimidazole → 1H-Imidazole, 1-(3-methyl-2-butenyl)-2-nitro-

HRID 1604125ノート

反応式

HRID 1604125 の反応式
[Na].[N+:2]([C:5]1[NH:6][CH:7]=[CH:8][N:9]=1)([O-:4])=[O:3].Br[CH2:11][CH:12]=[C:13]([CH3:15])[CH3:14]>C(#N)C>[CH3:14][C:13]([CH3:15])=[CH:12][CH2:11][N:6]1[CH:7]=[CH:8][N:9]=[C:5]1[N+:2]([O-:4])=[O:3]

参加物

5

反応物 3

HCID 107012-NitroimidazoleHCID 700922-Butene, 1-bromo-3-methyl-HCID 5360545Sodium

生成物 1

HCID 113443651H-Imidazole, 1-(3-methyl-2-butenyl)-2-nitro-収率 80%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To the sodium salt of 2-nitroimidazole prepared above was added acetonitrile (50 ml), 15-crown-5-ether (3.5 ml, 14.3 mmol) and 4-bromo-2-methyl-2-butene (2 ml; 17.4 mmol). The mixture was stirred at RT for ca 16 h. and then the solvent was removed to leave a crude semi-solid which was purified by column chromatography on silica. The intermediate product, 1-(3-methyl-2-butenyl)-2-nitroimidazole (80% yield) was eluted using a mixture of petroleum ether (40-60)/ethyl acetate (ratio 4:1 respectively).

後処理

  1. customthe solvent was removed
  2. customto leave a crude semi-solid which
  3. customwas purified by column chromatography on silica

出典と根拠

ORDレコード
ord-1d2032d9190244b6b46d78946d6a78e6
出典データセット
uspto-grants-1999_11
特許番号
US05993774

反応ノート

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